US3960585A - Reducing H2 S-emission from hot cast sulfur-asphalt mixtures - Google Patents

Reducing H2 S-emission from hot cast sulfur-asphalt mixtures Download PDF

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Publication number
US3960585A
US3960585A US05/529,429 US52942974A US3960585A US 3960585 A US3960585 A US 3960585A US 52942974 A US52942974 A US 52942974A US 3960585 A US3960585 A US 3960585A
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sulfur
asphalt
hydrogen sulfide
process according
composition
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US05/529,429
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William Gaw
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Shell USA Inc
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Shell Oil Co
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/06—Sulfur
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds

Definitions

  • the invention relates to an improved method of preparing cast sulfur-asphalt compositions wherein mixtures of sulfur and asphalt are mixed and/or heated at elevated temperatures to facilitate casting. More particularly, this invention is directed to a means for substantially suppressing the emission of hydrogen sulfide in the casting process described and to sulfur asphalt compositions containing agents which minimize hydrogen sulfide evolution at the high temperatures required for casting.
  • mixtures of sulfur, asphalt and mineral aggregate can be successfully cast into formed compositions such as pavements and construction articles, provided the sulfur and asphalt are present at a weight ratio of at least 1:1 sulfur to asphalt and the casting is carried out without the application of densification pressures.
  • the mixture should not be heated above 175°C in the casting process since above this temperature a chemical reaction between sulfur and asphalt takes place accompanied with emission of hydrogen sulfide.
  • the mixing temperature is 150°C or lower.
  • the instant invention provides an improved process for casting sulfur-asphalt compositions by mixing and/or heating mixtures comprising sulfur and asphalt at elevated temperatures not exceeding 175°C characterized in that the mixing and/or heating step is carried out in the presence of a hydrogen sulfide suppresant selected from the class consisting of free radical inhibitors, redox catalysts and mixtures thereof.
  • sulfur-asphalt compositons containing a hydrogen sulfide suppressant of the type described in an amount which is effective to substantially suppress hydrogen sulfide evolution from the sulfur-asphalt composition at temperatures up to 175°C.
  • the essence of the instant invention is the discovery that conventional free radical inhibitors and redox (oxidation-reduction) catalysts will effectively suppress the formation and/or evolution of hydrogen sulfide from mixtures of sulfur and asphalt which are heated to elevated temperatures required for casting without application of densification pressure, provided the temperature does not exceed 175°C.
  • suitable free radical inhibitors are tetra-alkylthiuram disulfide, zinc dialkyl dithiocarbamates and diphenyl guanidide.
  • Hydroquinone can also be used but is less suitable since it tends to sublimize and thus is easily lost from the system.
  • redox catalysts are iodine, copper salts and copper oxides, iron salts and iron oxides and cobalt salts and cobalt oxides.
  • the redox catalysts are generally preferred on a cost effectiveness basis.
  • the iron chlorides i.e., ferric chloride and ferrous chloride, appear to be the most effective and practical and are, therefore, preferred on that basis.
  • hydrated ferrous and ferric chloride i.e., FeCl 2 . 4 H 2 O and FeCl 3 . 6H 2 O, respectively.
  • hydrated ferrous chloride is the optimum additive for large scale applications, i.e., pavement casting, because of its superior effectiveness and non-corrosivity.
  • Combinations of free radical inhibitors and redox catalysts are also active hydrogen sulfide suppressants, for example a combination of copper carbonate and diphenylamine.
  • the particular amount of hydrogen sulfide suppressant which is added to the sulfur-asphalt composition to give the desired inhibiting effects at high temperatures is not considered to be at all critical to the invention and will vary considerably with the specific sulfur-asphalt composition employed, said composition generally also containing a mineral aggregate in addition to the sulfur and asphalt, and the extent to which hydrogen formation is to be suppressed.
  • the quantity of suppressant will only be a minor proportion of the total sulfur-asphalt composition with amounts as low as 0.05% by weight of the total composition being sufficient to give the desired suppressant effect.
  • the amount of suppressant will generally not exceed 0.5% by weight of the total composition, however, the use of larger amounts is by no means excluded from the scope of this invention should conditions warrant such use.
  • the temperature of the mixture containing sulfur and asphalt has some influence on the quantity of hydrogen sulfide which is emitted, a higher mixing temperature given a higher hydrogen sulfide emission.
  • the hydrogen sulfide suppressants according to the invention appreciably reduce the emission of hydrogen sulfide. It is preferred to use a mixing temperature of at most 150°C since at this temperature and below the quantity of hydrogen sulfide emitted can be reduced to negligible concentrations by using a hydrogen sulfide suppressant according to the invention.
  • the additives according to the invention be added to the asphalt component before it is mixed with the sulfur component.
  • the asphalt component when pavement compositions containing, for example graded mineral aggregate or sand, are being prepared and the asphalt and aggregate is mixed before the sulfur is added, it is preferred to add the suppressant to the minerals, the asphalt or to the mixture of asphalt and minerals, and to add the sulfur after the suppressant has been added.
  • the quantities of hydrogen sulfide emitted can still be significantly reduced by adding the additive after the sulfur in the mixing sequence.
  • Sulfur asphalt mixtures suitable for use in the invention comprise sulfur, asphalt and aggregate, the weight ratio of sulfur to asphalt being at least 1:1 and preferably from about 2:1 to 5:1 or higher.
  • Cast articles having sulfur to asphalt ratios of from 1.0:1 to 2.5:1 are particularly suitable as flexible pavements, while articles having ratios above 5:1 make suitable rigid pavements, blocks and the like. Cast articles having an intermediate ratio of 2.5:1 to 5:1 form very strong but still flexible pavements.
  • the sulfur employed in these mixes is elemental sulfur, that is, sulfur in the free state -- not as a compound. Any of the physical forms of sulfur are satisfactory for use because the sulfur is generally mixed with the asphalt in a molten state, although it is not necessary to do so.
  • Asphalt materials which may be suitably employed in these mixes include any asphalt generally used in road building, particularly pyrogenous asphalts derived from petroleum residues, e.g., residual oils, blown petroleum asphalt, soft and hard residual asphalt and the like. Other pyrogenous residues such as tar and pitch may also be used as well as mixtures of such materials with asphalt. Natural asphalt such as gilsonite may also be employed. Penetration grade asphalts, that is, those having a penetration (ASTM Method D 5) of 40-300, are particularly preferred. Asphalt is employed in the mix in an amount sufficient to bind the aggregate, e.g., generally at last 3% by weight of the total composition. Mixes containing from about 4 to 7% by weight asphalt are especially suitable.
  • the mineral aggregate used in the mix is generally defined as particulate inorganic matter and includes sand, stone, gravel, slag and the like, which may be either acidic or basic as in the case of granite and limestone, respectively. Because of its ready availability, sand of the conventional variety found on most construction sites is a preferred mineral aggregate for use in the instant invention.
  • FIG. 1 is a graph showing the quantity of hydrogen sulfide (vertical axis, logarithmic scale) released from the mix versus the total mixing time (horizontal axis, mg H 2 S/kg mixture/hour) at a mixture temperature of 143°C.
  • the upper curve shows the quantity of H 2 S using nitrogen as a carrier gas
  • the lower curve showing the quantity of H 2 S using air as the carrier gas. In both cases the flow rate of the carrier gas was 20 1/hr.
  • FIG. 2 is a graph showing the concentration of hydrogen sulfide in the reaction products as a function of time at different temperatures, viz. 182°C (curve A), 166°C (curve B), 160°C (curve C) and 143°C (curve D).
  • FIG. 3 shows a graph giving the relation of the quantity of hydrogen sulfide formed after 1 hour (vertical axis, logarithmic scale) and the reciprocal of the absolute temperature (horizontal axis). This graph was obtained from FIG. 2 by plotting the logarithm of the hydrogen sulfide concentration after 1 hour versus (absolute reaction temperature) - 1 .
  • FIGS. 1, 2 and 3 were obtained as follows.
  • Sulfur/asphalt/sand mixtures (composition 18/6/76%wt) were stirred in a temperature-controlled 2-liter glass reaction vessel.
  • the gaseous reaction products were carried to gas absorption bottles by a continuous stream of either nitrogen or air and analyzed for hydrogen sulfide.
  • a sulfur/asphalt/sand mixture (composition 18/6/76%wt) with added hydrogen sulfide suppressant was stirred in a temperature-controlled 2-liter glass reaction vessel.
  • the gaseous reaction products were carried to gas absorption bottles by a continuous stream of air at an air flow rate of 20 1/hr and analyzed for hydrogen sulfide.
  • the temperature of the mixture was 143°C.
  • the quantity of hydrogen sulfide measured is shown in Table I below.
  • Example II The experiments of Example I, while giving a good qualitative indication of the H 2 S suppressing action of additives according to the invention, are not quite representative for large-scale laying of pavement, since the continuous flow of air over a stirred mixture is not typical of commercial operations. Therefore, additional experiments were carried out on a larger scale and without air-flushing, in order to simulate mixture transportation and unloading. These experiments are described in Example II.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Working-Up Tar And Pitch (AREA)
US05/529,429 1973-12-17 1974-12-04 Reducing H2 S-emission from hot cast sulfur-asphalt mixtures Expired - Lifetime US3960585A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
UK58278/73 1973-12-17
GB58278/73A GB1494198A (en) 1973-12-17 1973-12-17 Reducing emission of hydrogen sulphide from hot mixtures containing sulphur and bitumen

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US3960585A true US3960585A (en) 1976-06-01

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US (1) US3960585A (da)
JP (1) JPS50105716A (da)
CA (1) CA1032704A (da)
DE (1) DE2459386C2 (da)
DK (1) DK138902B (da)
FR (1) FR2254609B1 (da)
GB (1) GB1494198A (da)
IT (1) IT1027727B (da)

Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4144082A (en) * 1977-11-17 1979-03-13 Chevron Research Company Sulfur plasticizing composition
US4210458A (en) * 1976-03-24 1980-07-01 Chevron Research Company Plasticized sulfur with improved thixotropy
US4283230A (en) * 1980-01-10 1981-08-11 Exxon Research & Engineering Co. Air-treated propane-precipitated asphalt
US4283231A (en) * 1980-01-10 1981-08-11 Exxon Research & Engineering Company Sulfur-treated propane-precipitated asphalt
US4339277A (en) * 1980-09-22 1982-07-13 Schult Hans E Solid sulfur-extended asphalt composition and method and apparatus therefor
US4559128A (en) * 1984-08-31 1985-12-17 Chevron Research Company Method for producing industrial asphalts
US4750984A (en) * 1985-11-18 1988-06-14 Ott Clifford J Method of producing asphalt
US6408683B2 (en) * 1998-06-15 2002-06-25 Wisconsin Alumni Research Foundation Laboratory asphalt stability test and apparatus
US20030075078A1 (en) * 2000-05-23 2003-04-24 Bailey William R. Paving binders and manufacturing methods
US6863724B2 (en) * 2001-08-09 2005-03-08 Shell Canada Limited Sulfur additives for paving binders and manufacturing methods
WO2005059016A1 (en) * 2003-12-10 2005-06-30 Shell Internationale Research Maatschappij B.V. Sulphur pellet comprising h2s-suppressant
EP1763562A2 (en) * 2003-12-31 2007-03-21 Fina Technology, Inc. Process for preparing bitumen compositions with reduced hydrogen sulfide emission
US20090206003A1 (en) * 2008-02-20 2009-08-20 Baker Hughes Incorporated Method for reducing hydrogen sulfide evolution from asphalt
WO2009121913A1 (en) * 2008-04-02 2009-10-08 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
WO2009121917A2 (en) * 2008-04-02 2009-10-08 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
US20110098385A1 (en) * 2008-04-08 2011-04-28 Total Raffinage Marketing Process for cross-linking bitumen/polymer compositions having reduced emissions of hydrogen sulphide
WO2011070446A1 (de) 2009-12-08 2011-06-16 Biothys S.A. (Societe Anonyme) Desodorierende formulierung
WO2011104726A1 (en) 2010-02-23 2011-09-01 Shell Internationale Research Maatschappij B.V. Bituminous composition
US20110290151A1 (en) * 2010-05-27 2011-12-01 Chughtai Majid Jamshed method providing for a low release of h2s during the preparation of sulfur-extended asphalt
RU2478592C1 (ru) * 2011-09-13 2013-04-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный строительный университет" Способ получения серобитумных композиций с пониженной эмиссией сероводорода и диоксида серы
CN103275498A (zh) * 2013-05-19 2013-09-04 新疆大学 改性硫磺颗粒及其制备方法和应用
RU2543838C1 (ru) * 2013-10-31 2015-03-10 МИНИСТЕРСТВО ОБРАЗОВАНИЯ И НАУКИ РОССИЙСКОЙ ФЕДЕРАЦИИ Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский автомобильно-дорожный государственный технический университет (МАДИ)" Способ производства асфальтобетонной смеси
US20180163050A1 (en) * 2013-11-12 2018-06-14 Total Marketing Services Bituminous compositions based on phosphoric derivatives
CN108795072A (zh) * 2018-06-08 2018-11-13 太原理工大学 一种替代部分沥青的硫基胶结料的毒物抑制剂及其使用方法
RU2732751C2 (ru) * 2018-06-29 2020-09-22 Общество с ограниченной ответственностью "Центр стратегических автодорожных исследований" Минерально-органический композит для защиты дорожных покрытий и способ его получения
US10920038B1 (en) 2018-08-03 2021-02-16 Dennis D. Krivohlavek And Lucindy June Krivohlavek Revocable Family Crosslink agent dispersible in oil or water for polymer modified asphalt
WO2021205465A1 (en) * 2020-04-06 2021-10-14 Hindustan Petroleum Corporation Limited Sulphur additive and sulphur modified bitumen

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2137633B (en) * 1983-03-31 1986-10-29 Exxon Research Engineering Co Decreasing h2s emission in bitumen/sulphur mixtures
US9346956B2 (en) * 2013-12-10 2016-05-24 Saudi Arabian Oil Company Foamed sulfur asphalts for pavement recycling and soil stabilization
CA2980404A1 (en) 2015-03-25 2016-09-29 Reliance Industries Limited A sulphur containing additive for making bitumen paving mixtures

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US491395A (en) * 1893-02-07 David a
US3738853A (en) * 1971-10-05 1973-06-12 Shell Oil Co Articles produced by casting of sulfur asphalt
US3803066A (en) * 1970-02-23 1974-04-09 Exxon Research Engineering Co Modifying bitumens
US3810857A (en) * 1970-11-20 1974-05-14 Petroles D Aquitaine Tour Aqui Bituminous compositions containing plastic or elastomer polysulphide polymers

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US491395A (en) * 1893-02-07 David a
US3803066A (en) * 1970-02-23 1974-04-09 Exxon Research Engineering Co Modifying bitumens
US3810857A (en) * 1970-11-20 1974-05-14 Petroles D Aquitaine Tour Aqui Bituminous compositions containing plastic or elastomer polysulphide polymers
US3738853A (en) * 1971-10-05 1973-06-12 Shell Oil Co Articles produced by casting of sulfur asphalt

Cited By (50)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4210458A (en) * 1976-03-24 1980-07-01 Chevron Research Company Plasticized sulfur with improved thixotropy
US4144082A (en) * 1977-11-17 1979-03-13 Chevron Research Company Sulfur plasticizing composition
US4283230A (en) * 1980-01-10 1981-08-11 Exxon Research & Engineering Co. Air-treated propane-precipitated asphalt
US4283231A (en) * 1980-01-10 1981-08-11 Exxon Research & Engineering Company Sulfur-treated propane-precipitated asphalt
US4339277A (en) * 1980-09-22 1982-07-13 Schult Hans E Solid sulfur-extended asphalt composition and method and apparatus therefor
US4559128A (en) * 1984-08-31 1985-12-17 Chevron Research Company Method for producing industrial asphalts
US4750984A (en) * 1985-11-18 1988-06-14 Ott Clifford J Method of producing asphalt
US6408683B2 (en) * 1998-06-15 2002-06-25 Wisconsin Alumni Research Foundation Laboratory asphalt stability test and apparatus
US20030075078A1 (en) * 2000-05-23 2003-04-24 Bailey William R. Paving binders and manufacturing methods
US6824600B2 (en) 2000-05-23 2004-11-30 Shell Canada Limited Paving binders and manufacturing methods
US6863724B2 (en) * 2001-08-09 2005-03-08 Shell Canada Limited Sulfur additives for paving binders and manufacturing methods
USRE44080E1 (en) 2001-08-09 2013-03-19 Shell Oil Company Sulfur additives for paving binders and manufacturing methods
WO2005059016A1 (en) * 2003-12-10 2005-06-30 Shell Internationale Research Maatschappij B.V. Sulphur pellet comprising h2s-suppressant
US20070125268A1 (en) * 2003-12-10 2007-06-07 Imants Deme Sulphur pellet comprising h2s-suppressant
AU2004299649B2 (en) * 2003-12-10 2008-05-22 Shell Internationale Research Maatschappij B.V. Sulphur pellet comprising H2S-suppressant
CN100471901C (zh) * 2003-12-10 2009-03-25 国际壳牌研究有限公司 包含h2s抑制剂的硫丸
US8025724B2 (en) * 2003-12-10 2011-09-27 Shell Oil Company Sulphur pellet comprising H2S-suppressant
EP1763562A2 (en) * 2003-12-31 2007-03-21 Fina Technology, Inc. Process for preparing bitumen compositions with reduced hydrogen sulfide emission
EP1763562B2 (en) † 2003-12-31 2019-06-26 Total Marketing Services Process for preparing bitumen compositions with reduced hydrogen sulfide emission
EP1763562A4 (en) * 2003-12-31 2011-10-19 Total Raffinage Marketing METHOD FOR PRODUCING BITUMEN MEASURES WITH REDUCED SULFUR HYDROGEN EMISSION
US20090206003A1 (en) * 2008-02-20 2009-08-20 Baker Hughes Incorporated Method for reducing hydrogen sulfide evolution from asphalt
US8034231B2 (en) * 2008-02-20 2011-10-11 Baker Hughes Incorporated Method for reducing hydrogen sulfide evolution from asphalt
EA017826B1 (ru) * 2008-04-02 2013-03-29 Шелл Интернэшнл Рисерч Маатсхаппий Б.В. Способ получения асфальта
WO2009121917A3 (en) * 2008-04-02 2010-04-22 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
AU2009232011B2 (en) * 2008-04-02 2011-06-09 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
WO2009121913A1 (en) * 2008-04-02 2009-10-08 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
US8557034B2 (en) 2008-04-02 2013-10-15 Shell Oil Company Process for manufacturing asphalt
CN102015569A (zh) * 2008-04-02 2011-04-13 国际壳牌研究有限公司 制备柏油的方法
US20110041732A1 (en) * 2008-04-02 2011-02-24 Jacques Colange Process for manufacturing asphalt
US20110041729A1 (en) * 2008-04-02 2011-02-24 Jacques Colange Process for manufacturing asphalt
WO2009121917A2 (en) * 2008-04-02 2009-10-08 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
AU2009232015B2 (en) * 2008-04-02 2012-05-17 Shell Internationale Research Maatschappij B.V. Process for manufacturing asphalt
EA017707B1 (ru) * 2008-04-02 2013-02-28 Шелл Интернэшнл Рисерч Маатсхаппий Б.В. Способ получения асфальта
US8202922B2 (en) 2008-04-08 2012-06-19 Total Raffinage Marketing Process for cross-linking bitumen/polymer compositions having reduced emissions of hydrogen sulphide
US20110098385A1 (en) * 2008-04-08 2011-04-28 Total Raffinage Marketing Process for cross-linking bitumen/polymer compositions having reduced emissions of hydrogen sulphide
WO2011070446A1 (de) 2009-12-08 2011-06-16 Biothys S.A. (Societe Anonyme) Desodorierende formulierung
US9028602B2 (en) 2010-02-23 2015-05-12 Shell Oil Company Bituminous composition
WO2011104726A1 (en) 2010-02-23 2011-09-01 Shell Internationale Research Maatschappij B.V. Bituminous composition
EA019659B1 (ru) * 2010-02-23 2014-05-30 Шелл Интернэшнл Рисерч Маатсхаппий Б.В. Битумная композиция
US20110290151A1 (en) * 2010-05-27 2011-12-01 Chughtai Majid Jamshed method providing for a low release of h2s during the preparation of sulfur-extended asphalt
US8361216B2 (en) * 2010-05-27 2013-01-29 Shell Oil Company Method providing for a low release of H2S during the preparation of sulfur-extended asphalt
RU2478592C1 (ru) * 2011-09-13 2013-04-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный строительный университет" Способ получения серобитумных композиций с пониженной эмиссией сероводорода и диоксида серы
CN103275498A (zh) * 2013-05-19 2013-09-04 新疆大学 改性硫磺颗粒及其制备方法和应用
RU2543838C1 (ru) * 2013-10-31 2015-03-10 МИНИСТЕРСТВО ОБРАЗОВАНИЯ И НАУКИ РОССИЙСКОЙ ФЕДЕРАЦИИ Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский автомобильно-дорожный государственный технический университет (МАДИ)" Способ производства асфальтобетонной смеси
US20180163050A1 (en) * 2013-11-12 2018-06-14 Total Marketing Services Bituminous compositions based on phosphoric derivatives
CN108795072A (zh) * 2018-06-08 2018-11-13 太原理工大学 一种替代部分沥青的硫基胶结料的毒物抑制剂及其使用方法
CN108795072B (zh) * 2018-06-08 2020-11-27 太原理工大学 一种替代部分沥青的硫基胶结料的毒物抑制剂及其使用方法
RU2732751C2 (ru) * 2018-06-29 2020-09-22 Общество с ограниченной ответственностью "Центр стратегических автодорожных исследований" Минерально-органический композит для защиты дорожных покрытий и способ его получения
US10920038B1 (en) 2018-08-03 2021-02-16 Dennis D. Krivohlavek And Lucindy June Krivohlavek Revocable Family Crosslink agent dispersible in oil or water for polymer modified asphalt
WO2021205465A1 (en) * 2020-04-06 2021-10-14 Hindustan Petroleum Corporation Limited Sulphur additive and sulphur modified bitumen

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Publication number Publication date
GB1494198A (en) 1977-12-07
DE2459386A1 (de) 1975-06-19
DK653474A (da) 1975-09-08
FR2254609B1 (da) 1978-12-22
DK138902C (da) 1979-04-30
DK138902B (da) 1978-11-13
JPS50105716A (da) 1975-08-20
IT1027727B (it) 1978-12-20
FR2254609A1 (da) 1975-07-11
DE2459386C2 (de) 1983-09-15
CA1032704A (en) 1978-06-13

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